Condensation dye from gallocyanins and process of making same.



UNITF D STATES .PATE

'BASEL, SWITZERLAND.

UT lFiiCill.

CONDENSATION DYE FROM GALLOCYANINS AND PROCESS 0.? MA'BZNG SAME.

Specification of Letters Patent.

Pzitented Sept. a, 1908.

Application filed April 21, 1908. 3eria1 No. 428,409.

To all whom it may cmwcm:

lie 1t known that we, CHARLES DE LA lIAnrE, chemist, .KARL Oswnno,chemist,

and ERNST Zsnxrxnn, doclor'ol"philosophy which the following u full,clear, and exact I specification.

It is known that the gullocynnins oblained by condensing nitrosocoinpounds with gullie acid and its deriw-"uliives curl be -('-)1nlcusedwith aromatic 21mins (molar or phlyulnins). The intermediate productsthus produced, which are little soluble or insoluble, urc generallyconverted by' sulfonution into new dyestuffs soluble in water. W'e havenow found that the said, non-sullonoled intermediateproducts, may beconverted, by suit able treatment with acids and reducing agents, intonew (lye-stuffs which dif-l'er sharply on) the'parent materials, thetreatz'rent with acids preceding or occompunying the reduction. Theyarevery easily soluble nwstcr and their aqueous solutions are nearlycolorless: dissolution rupidl .boeoines blue in an: With(Eonccntrnted suuric acid a green solution is obtained, whereas the nix-rent materialsand their leucmlerivntivcs dissolve in COIRCv'Qtlill'P-(l sulfuric acidto a). reddish solution; on mildition of an oxidant lilac M110 or K..Ur(),, the color of the solution does not change to blue,but remains gr-en and becomes after some time pale, the dyestufi being burned.

The new (lyestuil's are of great interest in res ect of their uplieu-lion to printing, sinec wit metallic inorr ants, especiallychromium mordnnts, they give very brilliant, pure blue tints of greatuniformity. lVit-h disclmrges a pure white is obtained. According totheir behavior they are not proper lcueo-derivatives of the parentmaterials, but the latter appear to be split up and reduced. At

all events the original mnin is to be detected in thehnother liquor.

Example I. parts of a gallocyanm-unilid, for inst-:inec the product ofthe action of :milin on the condensation product from nitroso-di'nielhylanilin and methylgullute are heated with 100 parts of alcohol of 96 percent. strength and parts of hydrochloric acid of per cent. strength ina. reflux apparatus on the water bath, and lhen is added in the courseof 3-4 hours zinc dust in small pol'ilmls until the original blue colorof the alcoholic solution has passed to yellowish green. and a sample nolonger dissolves in concentrated sulfuric acid to reddish violet, hut in:1 pure green solution. For this purnose nlmut- 4 ports of zinc dual.are needed. After cooling, lbe d esiull', whih sepnrates in greenishyellow needles is filtered and dried. in the mother liquorm1ilinc:men.-1- il nwognized. 'lhe dvestuil is easily soluble in purewater, the sulution being at lirst colorless and the). heron. up, blue.in l'eebly ucid water the solution remains colorless or fecblyYcllotvish. Who-r: prir rz-dcr; wool with chromium rnorri'znts, the=tull' yields a powerful, pure L-lue on being .umuedl Exninple H. 10ports of gullocymiiw :milid are suspended in 150 parts of alcohol, andufler addition of 3 part oi hydrochloric acid and 1 part of zinc dust,the whole is heated to feeble ebullition. purls of zinc O dustand24.nnrts of h \-drochloric acid are then added in ulterniite (loses,until u sample dissolv s in ()I1(:I1l'-\'r!l(ll sulfuric acid. ton puregreen solution. When r-nhl the d i'estull which precipitates ;isscpzzi"-r '.ul lronrthe mother liquor.

What we claim is:

1. The herein described process for the nuiuul'zicture of new dyestuflsby in uting the products rnzulc bycoudensing u gulloeynnin dyestull withan uronmiic :unin, with an acid and nreducing, agent.

2. As newdyeslnli's, the described derivali\-'es of the mulensurionproducts of gullocyzunn-dyestull's with aromatic umins, which are veryeasily soluhlein water, giving colorless solutions becoming rapidly,blue in air, dissolve in concentrated sulfuric acid with a greencoloration, which does not change on the addition of an oxidant but odesonly after some time, and give in. printing with metallicinorduntsbrilliant pure. blue tints of great uniformity. i

in testimony whereof, we have hereunto signed our names in the presenceof two subscribing witnesses.

CHARLES DE LA llAllPE.

S v ;hiJl). I ERNST Zlii i l'lhi l lll. Witnesszs:

AMAND Rrrrrm, (lso. (lurono.

